反応 #1501618

ord-70e0eb62538d40efac5979c168e51986

溶媒

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    その他The reaction pressure in the autoclave
  2. 2
    その他during the reaction
  3. 3
    その他After the ammonia was removed 30 ml of methanol
  4. 4
    workup.ADDITIONwas added to the reaction mixture for solvolysis
  5. 5
    workup.ADDITIONThereafter the product was treated in the same manner as in Example 2

実験手順

In a 200-ml autoclave were placed 26.6 grams (0.08 mole) of anhydrous sodium 1,5-naphthalene disulfonate, 17.6 grams (0.44 mole) of sodium amide and 80 ml of liquid ammonia in the same manner as in Example 1. The resultant mixture was heated at 180° C for 10 hours. The reaction pressure in the autoclave was 160 atm. during the reaction. After the ammonia was removed 30 ml of methanol was added to the reaction mixture for solvolysis. Thereafter the product was treated in the same manner as in Example 2, whereby 10.7 grams of 1,5-diaminonaphthalene was obtained. Yield was 84.5%.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US04001313uspto-grants-1977_01